CN101848863A - Methods of preparing clusterboron - Google Patents

Methods of preparing clusterboron Download PDF

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CN101848863A
CN101848863A CN200880114580A CN200880114580A CN101848863A CN 101848863 A CN101848863 A CN 101848863A CN 200880114580 A CN200880114580 A CN 200880114580A CN 200880114580 A CN200880114580 A CN 200880114580A CN 101848863 A CN101848863 A CN 101848863A
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acetonitrile
water
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hexane
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K·S·库克
M·奥克斯福德
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Semequip Inc
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00—Boron; Compounds thereof
    • C01B35/02—Boron; Borides
    • C01B35/026—Higher boron hydrides, i.e. containing at least three boron atoms
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
    • C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
    • C01B6/10—Monoborane; Diborane; Addition complexes thereof
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/30—Woven fabric [i.e., woven strand or strip material]
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Abstract

The invention provides new methods for synthesis of ClusterBoron (B18H22). Preferred methods of the invention include generation of the conjugate acid of B20H182, and decomposition of the acid in solution to generate B18H22 with high output and high purity. The invention further provides an isotope enriched boron hydride, especially an isotope enriched 10B18H22 and 11B18H22.

Description

The manufacture method of bunch boron
Technical field
The present invention system is about a kind of synthetic B 18H 22, become the miscellany of cis, trans-isomerism thing, be commonly referred to as the method for composite variety boron, form isotropic substance by the above-mentioned method of carrying and concentrate B 18H 22, particularly relevant for preparation natural abundance (natural abundance) B 18H 22, promptly 10The spissated B of B 18H 22And 11The spissated B of B 18H 22Manufacture method.
Background technology
The present invention advocates the right of temporary transient application case (Provisionalapplication) case that proposed on November 2nd, 2007 number 61/001685, and it is in full three according to being herein incorporated.
On semiconductor production, big hydroborates has become the important source material in the p type impurity district of doped with boron.Particularly preference for example is the hydroborates that comprises at least one Wuyuan submanifold boron with the high-molecular weight hydroborates, carries out the implantation of boron molecule as the raw material of boron atom.
The littler element faster of lasting exploitation is an important insight of modern semiconductor technology.Such process is called micro (scaling).Micro is by lasting progressive etch process method, makes that it can littler littler feature drives comprising on the semiconductor substrate of IC definition.Simultaneously, in the field of all semiconductor element designs, that is at various technology and micro node, the micro theory of general approval has developed into leads wafer to make in suitable replacement size (resize).Micro is the micro that connects the face degree of depth for the impact of ion embedding technology maximum, need increase shallow junction (shallow junction) when the dimension (dimension) of element reduces.The demand of increase shallow junction is transferred to following demand from the level of IC technology: at each section micro processing procedure, ion is implanted energy and all must be reduced.Extremely shallow junction need be known as the point 13 following microdevices of " supershallow connection surface (extremely shallow junctions) " or USJs now.
As the processing procedure of implanting,, therefore hindered the manufacturing that boron doped P type connects face with the boron ion owing to quite be difficult to control.Independent boron atom is very light (molecular weight=10.8), and it is dark excessively to penetrate silicon substrate, and can diffuse to the substrate lattice immediately in tempering (annealing) or other intensification processing procedures.
Bunch boron or cage boron for example are that borine is studied as transmitting the raw material of boron molecular species to semiconductor substrate, penetrate with minimizing.Please refer to PCT/US03/20197.
Big hydroborates is meant the boron compound that has between about 5 to 100 boron atoms, and preference is used in the ion implantation method of molecule, to transmit the boron atom in semiconductor substrate.Typically, may have the isomer existence of hydroborates.The meaning is meant that boron atom that hydroborates contains equal amts with hydrogen atom but have different chemical propertys, for example is Structural Isomerism thing or steric isomer.In addition, the hydroborates of two or more structurally associateds contains the boron atom of equal amts but the hydrogen atom of different quantities has been separated into bunch boron of various different sizes.For instance, each other molecular formula of five borines (9) and five borines (11) is B 5H 9And B 5H 11Such compound is categorized into closed type (closo, B usually nH n), nido (nido, B nH N+2), spider web (arachno, B nH N+4), spacious net (hypho, B nH N+6), connection formula (conjuncto, B nH N+8) and analogue.Therefore, the compound that different borine kinds comprises isomer and contains the different hydro atomic quantity often is regarded as having the borine of n boron atom.James (Jimmis) and other people provide the various overviews that condense the compound of type borine (macropolyhedral boranes) and the known n of having boron atom and different hydro atomic quantity 1,2
The mixture of isomer and suitable the use on the method for implantation of being discussed of mixture with borine of n boron atom.The molion that the hydroborates mixture is produced by the ionization processing procedure (molecular ions) has consistent and narrow and small molecular weight distribution.
At present the synthetic technology of the hydroborates molecule that preparation is big for example is the hydroborates molecule with 12 boron atoms, is often perplexed by the synthetic processing procedure of complexity, low isolated yield and the reproducibility of (perhaps) inconsequent.
Though, mention many fixed synthesis modes in the literature and be used to prepare B as isomer mixture 18H 22, but method is very tediously long, and often causes apparent low yield, so these synthesis modes are unreliable and security concerns are arranged.
Therefore, yearning can accessing prepares B 18H 22Novel method.
Summary of the invention
We have found a kind of preparation 18 borines (octadecaborane, B 18H 22) novel method.The present invention is specially adapted to easy synthetic and a large amount of B 18H 22Purifying.The present invention also concentrates B relevant for isotropic substance 18H 22Yet,, concentrate the meaning of the natural abundance change that is meant boron istope from definition.According to the difference in source, 10B natural abundance of isotopes scope from 19.10% to 20.31%, and 11B natural abundance of isotopes scope from 80.90% to 79.69%.
Typical B 18H 22It is to lose caused variation of quantity by hydrogen atom from molion that molecular ion beam has comprised large-scale mass of ion, and caused by the caused variation of quality of isotropic substance of two natural generations.Carry out mass separation by make employed implanted device at semi-conductor, be used in B 18H 22Isotropic substance concentrate the dispersion that boron can reduce quality significantly, thereby implant kind at needed ion, a kind of enhanced ion beam current is provided.Therefore, also relevant for 10B and 11The isotropic substance of B concentrates B 18H 22
Implement aspect one, the invention provides a kind of synthetic manufacturing 18 borine (B 18H 22) novel method, this method may further comprise the steps, and (a) makes borine negatively charged ion B 20H 18 2-In solvent, contact, produce H with acid 2B 20H 18XH 2O solution; (b) with water and/or residual solvent by spissated H 2B 20H 18XH 2Remove in the O solution; And (c) separate B 18H 22Say rightly, with water and/or residual solvent by spissated H 2B 20H 18XH 2Remove in the O solution and can promote B 18H 22Formation.
Certain enforcement aspect of the present invention provides a kind of synthetic B 18H 22Method, comprise the following steps:
(a) make borine negatively charged ion B 20H 18 2-In solvent, contact, produce H with acid 2B 20H 18XH 2O solution;
(b) the concentrated H that contains 2B 20H 18XH 2The mixture of O;
(c) with water and residual solvent by spissated H 2B 20H 18XH 2Remove in the O solution, promote B 18H 22Formation;
(d) resistates that is produced is dissolved in the biphase mixture, makes the by product of reaction and unreacted material dissolves in a kind of solvent composition wherein, B 18H 22Be dissolved in second kind of solvent composition;
(e) B will be contained respectively 18H 22And each layer of by product separately;
(f) isolate highly purified B by suitable cleaning 18H 22, drying also removes solvent;
(g) necessary, reclaim by product.
Above-mentioned step finds expression in the 2nd figure in the mode of schema.Preferred methods of the present invention is applicable to the B of preparation isotropic substance purifying 18H 22And B 18H 22The mixture of Structural Isomerism thing.In other words, the invention provides the B that can produce the suitable molecular ion beam that is fit to the ion implantation 18H 22
In some enforcement aspect of the present invention, with B 20H 18 2-The B of salts solution 20H 18 2-Negatively charged ion contacts with acid, produces H 2B 20H 18XH 2O solution, and concentrate by the mode that removes primary solvent.Solvent or mixed solvent are with B 20H 18 2-Salt and H 2B 20H 18XH 2O is all solvable but can not destroy the two for good.The solvent of this class or mixed solvent comprise water, alcohols, nitrile, ethers, cyclic ethers class, sulfone class (sulfones) and analogue.
In some enforcement aspect of the present invention, acid is can be to replace B 20H 18 2-The protonated B of the mode of cationic salts 20H 18 2-Bunch mineral acid.The preferably be pKa less than 2, include but not limited to spirit of salt, sulfuric acid, nitric acid, Hydrogen bromide, hydroiodic acid HI, sulfurous acid and selenic acid.
In some enforcement aspect of the present invention, acid is can be to replace B 20H 18 2-The protonated B of the mode of cationic salts 20H 18 2-Bunch organic acid.The preferably be pKa less than 2, include but not limited to trifluoromethane acetate (trifluormethaneacetic acid), trifluoroacetic acid, Phenylsulfonic acid, oxalic acid, tosic acid (p-toluenesulfonic acid), trichoroacetic acid(TCA) and dichloro acetic acid.
In some enforcement aspect of the present invention, acid is any can all being suitable for using at synthetic B provided by the present invention with the anionic acidic ion exchange resin of proton (protons) exchange borine 18H 22Method in.Preferable acidic ion exchange resin comprises crosslinked (cross-linked), solvent soluble (solvent-insoluble) resin, has a plurality of acid functional groups, can be with the negatively charged ion of proton exchange borine salt.Some preferable acidic ion exchange resin comprises having a plurality of sulfonic aromatics or the polymkeric substance of partially aromatic, comprises that the polymkeric substance that for example has crosslinked aromatics or partially aromatic is for better.
By spissated H 2B 20H 18XH 2Remove unnecessary solvent and water in O (wherein x the is a positive number) solution with output B 18H 22Though wish not limited to by theory, actual situation is by in the aqueous H30 hydroxonium ion alite, and the solvent removal of water or other crystallizations is guided H 2B 20H 18XH 2O is suitable for causing the degraded of a part of oxonium ion.The preferable degraded situation of typical case comprises the use vacuum drying oven, dry inert gas bundle (dry inert gas streams) or make aqueous H30 hydroxonium ion alite contact one or more siccative, for example molecular sieve, Vanadium Pentoxide in FLAKES, alumina, silica, silicate and analogue or its combination.Can promote by the temperature range that removes water in the system between about 0 ℃ to about 250 ℃.
In some enforcement aspect of the present invention, can be by multilayer mixed solvent solubilizing reaction resistates.The extraction B of mixed solvent optional 18H 22Extremely wherein one deck can separate product swimmingly.By product and remaining B 20H 18 2-Class is extracted to the second layer and is not decomposed, and therefore can reclaim B 20H 18 2-Material.Preferable mixed solvent includes but not limited to acetonitrile/hexane, acetonitrile/hexanaphthene, water/hexane, water/hexanaphthene, acetonitrile/benzene, water/benzene and water/toluene.
In preferable enforcement aspect, the invention provides synthetic B 18H 22Method, comprise the following steps:
(a) make boron anion B 20H 18 2-At acetonitrile: contact with acidic ion exchange resin in the water mixed solvent, produce H 2B 20H 18XH 2O solution;
(b) the concentrated H that contains 2B 20H 18XH 2The mixture of O;
(c) by use 30 ℃ to 55 ℃ vacuum drying oven with water and solvent by removing in the reaction mixture;
(d) with acetonitrile: the biphasic solvent mixture extraction of hexane goes out resistates;
(e) hexane layer is separated from acetonitrile layer;
(f) clean hexane layer with acetonitrile, clean with water again, and by removing or the mode of concentrated hexane solution is isolated B 18H 22
(g) also clean according to the step process acetonitrile layer of (a) to (f).
Preferred approach of the present invention is fit to provide at ion implants the B that can produce suitable molecular ion beam 18H 22With other industrial application.In comprising that ion is implanted in, most of present or possible application is with the B of aforesaid method manufacturing 18H 22Avoid main metallic pollution and do not need further purifying, for example concise or recrystallize.
The synthetic method provides the B of high score from productive rate (＞50%) with less synthesis step 18H 22, be applicable to that the preparation isotropic substance concentrates B 18H 22, for example 10The isotopes concentration of B be 50% or above and 11The isotopes concentration of B greater than 90% or more than.Synthetic method of the present invention can actually be used the pure isotropic substance B of preparation 18H 22Or isotropic substance concentrates 10B reaches 11The B of B 18H 22, a part is owing to less synthesis step, (＞60% by B for quality efficiency (mass efficiency) and high total synthetic productive rate 20H 18 2-).
Disclose as follows about other embodiments of the present invention.
Description of drawings
Fig. 1 is the schema of the preferable implementation step of the present invention.
Embodiment
Fig. 1 is the step of preferred embodiment of the present invention.
In the method for the present invention 10The isotopes concentration of B atom is to be good greater than natural abundance, for example in product B 18H 22In the boron atom that exists at least about 50% be 10B, or in product B 18H 22In the boron atom that exists at least about 80% be 10B, or in product B 18H 22In the boron atom that exists at least about 90% be 10B, or in product B 18H 22In the boron atom that exists at least about 95% be 10B, or in product B 18H 22In the boron atom that exists at least about 99% be 10B.
In the method for the present invention 11The isotopes concentration of B atom is to be good greater than natural abundance, for example in product B 18H 22In at least about 90% boron atom be 11B, or in product B 18H 22In at least about 95% boron atom be 11B, or in product B 18H 22In at least about 99% boron atom be 11B.
The present invention up to the present only summary describe, for can clearer understanding the present invention, enumerate following example, comprise with explanation the present invention be purpose enumerate the time execute aspect and embodiment, but be not in order to limit the present invention.
Embodiment
With (HNEt 3) 2B 10H 10(400.0g 1.24mol) is dissolved in the water of the acetonitrile of 3L and 500mL, preparation recrystallize but undried (HNEt 3) 2B 20H 18XH 2O.Then come IR-120 acidic ion exchange resin tubing string to contact solution and the peace hundred of 10kg.Acetonitrile washing H with other 3L 2B 20H 18XH 2O solution then launches and cleans binding substances.Enriched mixture is to form sticky shape xanchromatic oil and to move on the glass tray.The glass tray is placed 40 ℃ of vacuum drying ovens and is in the dynamic vacuum state.Remove superfluous solvent and water, can observe gaseous volatilization and solid-state resistates slowly forms.Acetonitrile/hexanes mixtures (750ml/2L) extracted residues with two-phase.The xanchromatic acetonitrile layer is separated and is placed by hexane layer on one side.Necessary, can make separation more smooth and easy by filtering out in the mixture insolubles in advance.(2 * 200mL), (3 * 200mL) clean hexane layers and with the magnesium sulfide drying to water with acetonitrile.Under vacuum, remove hexane, stay the B of white 18H 22(76.5g, 56.9% from B 10H 10 2-).Though be not the output that must reach high, acetonitrile layer and acetonitrile scavenging solution are mixed and be exposed to the acidic exchange tubing string.Form with above-mentioned identical method and separate B 18H 22(raw material that 12.8g is unnecessary, ultimate production 89.3g, 66.4%).
The present invention describes in detail by its preferred embodiment.Yet, be familiar with related art techniques person of the present invention, can in spirit of the present invention and field, be improved according to the part that has disclosed.
Reference:
1?Jemmis，E.D.；Balakrishnarajan，M.M.；Pancharatna，P.D.，ElectronicRequirements?for?Macropolyhedral?Boranes.Chem.Rev.2002，102，93-144.
2.Jemmis，E.D.；Balakrishnarajan，M.M.；Pancharatna，P.D.，AunifyingElectron-Counting?Rule?for?Macropolyhedral?Boranes，metallaboranes，andMetallocenes.J.Amer.Chem.Soc.2001，123，4313-4323.
3.Pitochelli，A.R.；Hawthorne，M.F.，The?Preparation?of?a?New?Boron?HydrideB 18H 22.J.Amer.Chem.Soc.1962，84，3218.
4.Hawthorne，M.F.；Pilling，R.L.；Stokely，P.F.，The?preparation?andrearrangement?of?the?three?isomeric?B20H184-ions.J.Am.Chem.Soc.1965，87，1893-1899.
5.Olsen，F.P.；Vasavada，R.C.；Hawthorne，M.F.，The?chemistry?of?n-B18H22and?i-B18H22.J.Am.Chem.Soc.1968，90，(15)，3946-3951.
6.Chamberland，E.L.；Muetterties，E.L.，Chemistry?of?Boranes.XVIII.Oxidation?of?B10H10-2?and?its?derivatives.Inorg.Chem.1964，3，1450-1456.
In these all patents quoted and publication usefulness as a reference.
This area related art techniques person can recognize or only just can understand with general experience, described in certain embodiments of the invention equipollent (equivalents).These equipollents are contained in following claims.

Claims (42)

1. one kind is synthesized 18 borine (B 18H 22) method, this method comprises the following steps:
(a) make borine negatively charged ion B in the solvent 20H 18 2-Contact with acid, thereby produce H 2B 20H 18XH 2O solution;
(b) with water and/or residual solvent by spissated H 2B 20H 18XH 2Remove in the O solution;
(c) separate B 18H 22
2. the method for claim 1, wherein with water and/or residual solvent by H 2B 20H 18XH 2Remove in the O solution and promote B 18H 22Formation.
3. one kind is synthesized 18 borine (B 18H 22) method, this method comprises the following steps:
(a) make borine negatively charged ion B in the solvent 20H 18 2-Contact with acid, thereby produce H 2B 20H 18XH 2O solution;
(b) the randomly concentrated H that contains 2B 20H 18XH 2The mixture of O;
(c) with water and residual solvent by H 2B 20H 18XH 2Remove in the O solution;
(d) randomly the gained resistates is dissolved;
(e) preferably separation contains B 18H 22With the layer that contains by product;
(f) B of separating high-purity 18H 22
(g) randomly reclaim byproduct layer.
4. method as claimed in claim 3 is wherein handled resistates with biphase mixture in optional step (d), in described biphase mixture, byproduct of reaction and unreacted material dissolves are in a kind of solvent composition, and B 18H 22Be dissolved in second kind of solvent composition.
5. method as claimed in claim 3, wherein in step (f) by clean, dry and/or remove the pure B of separated from solvent 18H 22
6. as claim 1,2 or 3 described method, wherein B 20H 18 2-Salt is [NR for the positively charged ion formula 1R 2R 3R 4] +Alkylammonium salt, wherein
R 1, R 2And R 3Be independently selected from hydrogen, C 1-20Alkyl, C 6-10Aryl, C 7-10Aralkyl, perhaps R 1, R 2Or R 3Any both in conjunction with forming heterocycle; And
R 4Be selected from hydrogen, C 1-20Alkyl or C 6-10Aryl.
7. as claim 1,2 or 3 described methods, wherein should acid be pKa less than about 2 organic acid.
8. as claim 1,2 or 3 described methods, wherein should acid be pKa less than about 2 mineral acid.
9. as claim 1,2 or 3 described methods, should acid be acidic ion exchange resin wherein.
10. method as claimed in claim 9, wherein this acidic ion exchange resin is aromatics or the partially aromatic polymkeric substance that comprises a plurality of sulfonic acid resistatess.
11. method as claimed in claim 9, wherein this acidic ion exchange resin is cross-linked polystyrene.
12. as claim 1,2 or 3 described methods, wherein this solvent is the mixture of water-based and non-aqueous solvent.
13. method as claimed in claim 12, wherein this non-aqueous solvent is selected from alcohol, nitrile, ether or its combination.
14. method as claimed in claim 12, wherein this non-aqueous solvent comprises methyl alcohol, ethanol, acetonitrile, tetrahydrofuran (THF), dioxane or its combination.
15. method as claimed in claim 12, wherein this non-aqueous solvent comprises the acetonitrile of about 1 volume % to about 99 volume %.
16. method as claimed in claim 12, wherein this non-aqueous solvent comprises the acetonitrile of about 80 volume % to about 95 volume %.
17. method as claimed in claim 12, wherein this non-aqueous solvent is an acetonitrile.
18. method as claimed in claim 12, wherein this solvent comprises the water of about 1 volume % to 99 volume %.
19. method as claimed in claim 12, wherein this solvent is about 6: 1 acetonitrile of by volume: the mixture of water.
20. as claim 1,2 or 3 described methods, wherein by using vacuum, dry inert gas or as the siccative of molecular sieve, Vanadium Pentoxide in FLAKES, alumina, silica, silicate etc., or its combination removes water.
21. as claim 1,2 or 3 described methods, wherein by using vacuum drying oven to remove water.
22. as claim 1,2 or 3 described method, wherein B 18H 22Be formed on about 0 ℃ and take place to about 250 ℃ temperature.
23. as claim 1,2 or 3 described method, wherein B 18H 22Be formed on 20 ℃ and take place to about 50 ℃ temperature.
24. method as claimed in claim 3, wherein this biphasic solvent system is selected from water, nitrile, alcohol, ether, alkane, aromatic hydrocarbons, naphthenic hydrocarbon or its combination.
25. method as claimed in claim 24, wherein this biphasic solvent system is an acetonitrile: hexane.
26. method as claimed in claim 24, wherein this biphasic solvent system is an acetonitrile: hexanaphthene.
27. method as claimed in claim 3 wherein reclaims byproduct layer and carries out 0 time.
28. method as claimed in claim 3, wherein repeating step (a) to (f) once.
29. method as claimed in claim 3, wherein repeating step (a)-(f) surpasses once.
30. synthetic 18 borine (B 18H 22) method, this method comprises the following steps:
(a) make at acetonitrile: the borine negatively charged ion B in the solvent mixture of water 20H 18 2-Contact with acidic ion exchange resin, thereby produce H 2B 20H 18XH 2O solution;
(b) the concentrated H that contains 2B 20H 18XH 2The mixture of O;
(c) by use 30-55 ℃ vacuum drying oven with water and solvent by removing in the reaction mixture;
(d) use acetonitrile: hexane biphasic solvent mixture extraction reaction residue;
(e) separate hexane layer by acetonitrile layer;
(f) clean hexane layer with acetonitrile, water cleans hexane layer again;
(g) by removing or concentrated hexane solution separation B 18H 22
(h) handle acetonitrile layer and washings according to step (a)-(g).
31. synthetic 18 borine (B 18H 22) method, this method comprises the following steps:
(a) make acetonitrile: the borine negatively charged ion B in the solvent mixture of water at 6: 1 20H 18 2-Come acidic ion exchange resin to contact with peace hundred, thereby produce H 2B 20H 18XH 2O solution;
(b) the concentrated H that contains 2B 20H 18XH 2The mixture of O;
(c) by use 40 ℃ vacuum drying oven with water and solvent by removing in the reaction mixture;
(d) use acetonitrile: hexane biphasic solvent mixture extraction reaction residue;
(e) separate hexane layer by acetonitrile layer;
(f) clean hexane layer with acetonitrile, water cleans hexane layer again;
(g) by removing or concentrated hexane solution separation B 18H 22
32. synthetic 18 borine (B 18H 22) method, this method comprises the following steps:
(a) make acetonitrile: the borine negatively charged ion B in the solvent mixture of water at 6: 1 20H 18 2-Come acidic ion exchange resin to contact with peace hundred, thereby produce H 2B 20H 18XH 2O solution;
(b) the concentrated H that contains 2B 20H 18XH 2The mixture of O;
(c) by use 40 ℃ vacuum drying oven with water and solvent by removing in the reaction mixture;
(d) use acetonitrile: hexane biphasic solvent mixture extraction reaction residue;
(e) separate hexane layer by acetonitrile layer;
(f) clean hexane layer with acetonitrile, water cleans hexane layer again;
(g) by removing or concentrated hexane solution separation B 18H 22
(h) use acetonitrile layer and acetonitrile washings repeating step (a)-(g) at least once.
33. as the described method of claim 1 to 32, wherein 10The isotopes concentration of B atom is greater than natural abundance.
34. method as claimed in claim 33, wherein product B 18H 22In the boron atom that exists at least about 50% be 10B.
35. method as claimed in claim 33, wherein product B 18H 22In the boron atom that exists at least about 80% be 10B.
36. method as claimed in claim 33, wherein product B 18H 22In the boron atom that exists at least about 90% be 10B.
37. method as claimed in claim 33, wherein product B 18H 22In the boron atom that exists at least about 95% be 10B.
38. method as claimed in claim 33, wherein product B 18H 22In the boron atom that exists at least about 99% be 10B.
39. as the described method of claim 1 to 33, wherein 11The isotopes concentration of B atom is greater than natural abundance.
40. method as claimed in claim 39, wherein product B 18H 22In the boron atom that exists at least about 90% be 11B.
41. method as claimed in claim 39, wherein product B 18H 22In the boron atom that exists at least about 95% be 11B.
42. method as claimed in claim 39, wherein product B 18H 22In the boron atom that exists at least about 99% be 11B.
CN200880114580A 2007-11-02 2008-11-03 Methods of preparing clusterboron Pending CN101848863A (en)

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JP5710975B2 (en) 2015-04-30
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JP2011502923A (en) 2011-01-27
EP2212251B1 (en) 2016-12-21
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US20110165053A1 (en) 2011-07-07
WO2009058406A1 (en) 2009-05-07

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